Process for the manufacturing of gray acetate of lime and wood-alcohol.



No. 886,183. PATENTED APR. 21, 1908.

4 H.. B. SCHMIDT. PROCESS POR'THB-MANOPACTORE OP CRAY ACETAT'B OF LIME AND WOOD ALCOHOL.

' APPLICATION FILED PEB. 12, 1902.

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JMKCM UNITED sTAfrnsrATENT OFFICE.

HERMAN B. SCHMIDT, OFV CINCINNATI, OHIO, ASSIGNOR TO.: JOSLIN, SCHMIDTdz (30,013V

CINCINNATI, OHIO, A FIRM.

PROCESS -Fon'rnn MAN'UFACTURE on GRAY ACETATE oF LIME AND Woola-amazon.l

Nq.vss5,183.

, Applieation mea February 121902. serial Naeaesa Cincinnati, conty...offI-I amilton, State 'of tion.

Ohio, have inventedrv certainnew and useful Improvements in Processesfor-theManufacj ture of Grayk'Acetate ofLimeand Wood-Alcohol, of W This invention relates-to processes for the manufacture of gray acetate of lime and wood alcohol.

The object of the invention `is the rovision of a process for the manufacture` o gra acetateo lime andwood alcoholwhich W beeconomical in the use of labor and steam,

vand Water for condensation pur oses, yand will insure the production of lwoo alcohol inf -any desired proof, ina rapid manner and combine in' one process what has heretoforei required distinct and independent processes to accomplish. s

form of apparatus to accomplish-it.

a The novel features of the process are .set

l forth in the appended claims.

pyroligneous In' the drawlng': Figure 1 is a-i'epresentation-` of a preferred form of apparatusfon carryingI out the form of one of t e alcohol columns.

A re resents a still suppled with/suitablesteam` eating. coils A intowhichthe" crude eatlng coils setto boilin From this lng throu h pipe Q they are dischar e into tank B. n the tank B, is placed a c argeof quicklime, immersed in water or in weak acid liquors obtained from` tar distillation. Weak acid liquors are employed, because the small amount of volatile acetic, etc. acids in the solution after neutralization with' lime would not ay to evaporate by itselfas thej cost.of fue would exceed the valu"e of the acetate of lime recovered;v therefore, vthese weak acid li uorsare used instead-of water to make a m k of lime, which on bein saturated with the volatile acids in the st after evaporation, yields an increased amount of acetate of lime. The lime absorbs the acid vapors and the alcoholic vapors and steam Specification of Letters Patent.

ich the following is a speciica-- C being y`.t y. a p1pe O and tank F by a ipe P leadrocess;Fig. 2 is a. modied" li mg into the lower (por containing2% alcohol pumped throu pipe 1 `and by means ofthe .Patented April 1908;

rise through a. column G,vsurrounding piple Q and ass via p'ipe'Gr into aseparator Where a matter mechanically carried over is deposited `in the lime solution again. The vapors are then carriedthroughdpipe apipe 'I havingl thje valves'V an and an extension pipe 'J opening into theair and- Bintov ted toA be used as yan exhaust and then` pors in- 'columnK `are met vby a descendingA column of weak alcoholic liquor (test from' 1 to 5 alcoholic strength on the alcoholometer) supplied by a pump S and pipe S sprayed adapl disc arge into a columnK. The rising ,v a.

into .the upper portion of column K, andthe non-condensed portion of the ,rising Va or is carried to .a condenser`N via pipe and passes" from the 'condenser into a storage?v tank Ng vof suitable form and dimensions.

The condensed vliquor from column K passes through a tail pipe K into a tank D, from which it flows into a receiver E and is then C, located below tank- B, or from a tank F,

containing oil and water tailings the receiver 1n communication with column L ortion o column L.

, p forced by pressuregfrom pipe E received The process is set forth fully hereinafter and described in connection with a preferre` d v The acetate of,` lime so ution in C occasionally vfurnishes alcohol, forf the reason that if the operatives, are careless in not having an excess of lime present in B, then the methyl acetate vapors are not decomposed by the lime then these can be boiled overfrom tank C; they will practically vapor of Water is given ff from it.

fdesired, a boiling Ipipe T may be laced in the bottom of column as indicate in Fig. 2 to generate vapor from the liquor in the bottom vof said column L. The vaporous alcohol is condensed in another condenser M and conducted to a suitable tank M', while the tailings p aass 'from column L intotank F via a P1P@ As a generalrule the tank F con- `then go into the alcohol columnL and be tains only Water and oils which can be discharged therefrom into a sewer, but as a recautionary measure against wasting alco ol, the li uor in tank F can beset to boiling by use of steam pipe Z and the distillate condensed and tested for alcohol. The. precautionary measure against wasting alcohol is stated in the following clause: the liquor ,in tank F'can be set boiling, and the distillate l1() going off through pipe Pinto the alcoholic column L would indicate a higher percentage of alcohol, vwhich condensed in M would show at the tail box M It is of course understood, that during this operation no liquor from the 15 Iweak alcoholic tank E must be discharged,

through the'pipe U on top of the column L. Such acourse is far more satisfactory than to cool a sample from the tank F and test it di rectly, as I have found `that While the tailin s may show no test for alcohol on an alcoho ometer, yet when submitted to distillation, they give a perceptible show of alcohol, probably 2% ior more. In order that the tank F may contain 'only Water and oils, the tail 25 boxes should be watched so that nothing but water is discharged from the bottom of the i column. This can be re ulated very easily, by`having the Weak alcoolic vapor from VE oing through pipe U onto the top of the alco- 3oI ol column L- so regulated, that only water and oil comefrom the'base of the column. YPipes-Z, Z and Z, are steam pipes-for boiling the contents or for creating pressure in .the res ective tanks F, D, C.

' he boiling vof the.p roli neous liquor in still A is continued unti the lime in tank Bis two-thirds neutralized more or less, When the l feedin of Weak alcohol through ump S into the column K is ystopped and tlie distillate 40 through condenser M is tested. When the distillation in still A has been arrested, after valve W in pipe J is opened and the valve VV closed and the boiling of the liquor in A continued, thus discharging only vapor of Water through the pipe J into the outside air. This is continued until the lime in tank B shows that it is saturated, when acetate of lime is formed, the formula being as follows at which time the operation is sto ped and the contents of tank B are droppe into receiver C, when they give off 78 hol, in vapors, through pipe O. The tank B is then recharged with dry lime and liquor to. 80? alcoand the operation is continued. The noW saturated acetate liquor is discharged from the receiver C through pipe X, by suitable pressure received from ipe 2, into settling tubs into which the said) pipe discharges, or through a filterpress yto separate the insoluble lime compound from the liquor containingthe soluble acetate oflime. By the ,above operations the liquor in tank B can be brought to a saturated solution with the steam necessary to evaporate the' original pyroligneous liquor. If it were not for the ac t that the vinsoluble matter mustbe separated to make a good gray acetate, the saturation and evaporation of the liquor in tank B might be brou ht to any deslred degree, but onfthe other and, if the liquor in tank B shows the lime to be saturated and the condensed liquor from condenser N shows alcoholic proof, then the boiling of the liquor in still A should be stopped and the liquor in tank B discharged into the receiver C, after the lime is all neutralized by the acetate acid. The condensed alcohol vapors in tank E are forced to the to of column L to save evaporation in tank This weak alcohol in bein forced to the top of column L is separatecgl out by the ascending currents of steam from the boiling of the contents of the tank F and the vaporsA from tank C. Thecondenser N discharges alcohol testing from 97% to start with down to about 78% to finish with, making the average test about 85% for about three quarters of the operation and the balance' which runs y from 78% to nothing is again run into the tank D to start the next operation.` The ndenser M yields a small amount of alcohol of an average test of 85% strength and a relatively large amount of weak alcohol which may'run from 2% to 7% which is run into asuitable tank and then to storage tank lF to start the next operation.

It 1s advantageous to (so arrange the lime charges that the alcoholicl test is off at condenser before the lime is saturated in the tank B. In this wa the excess of water in still A is discharge as vapor through the pipe J into the outer airand is not carried through'theapparatus and condensed and so dilute the strength of the alcoholic distillate. Itis desirable to have the yroligneous li uor discharged into the top of) the column Qqbefore entering the still A. In this way a large percentage of the alcoholic strength is prevented from gettin into still A, so that after the feeding of the liquor into the column (.is stopped thealcohohc strength in still A c `n be oiled out much sooner and can al- -ways be so regulated that the excess of lime enabled to accomplish in one operation what has formerly required independent and distinct processes and also to effect a multiple use of the steam which, obviously is a matter of great economy. Also it is possible to obtain alcohol of any higher proof as desired.

I am aware that other forms of apparatus miht be employed to carry out the process, an I do not, therefore, restrict myself to the use of the apparatus herein shown and de scribed. y

Having thus described my invention what I claim as new and desire to secure by Letters Patent, is:

`1. A process of manufacturing consisting in converting crude pyroligneous liquor in to vapors, extracting or eliminating, y i the acid vapors resulting from such treatment and subjecting the resulting vapors ol"v l' .fi water and alcohol to the action of weak alcoholic solutions and thereby obtaining an i alcohol, Y

alcoholic solution of any desired -higher proof.

2. A process of manufacturing alcohol, consistingV in boiling or 'eva orating crude 1 pyroligneous liquor, passing t e vapors prog duced by 'such treatment through a lime solution to absorb the acid vapors, and evapol rating .the alcohol from Weak alcoholic .solul tions by bringing the same into the presence of the alcoholic and water` vapors remaining f at the elimination of the acid vapors by the 1 lime solution and thereby obtaining an alcoholic solution of any desired higher proof without further use of the steam.

In testimony whereof I hereunto al'i'x my signature in presence of two witnesses.

HERMAN' B. SCHMIDT.v

Witnesses: l

GRAFTo.\ TYLER,

FRED CL'Oss. 

